Alicia Vallet , Isabel Ayala , Barbara Perrone , Alia Hassan , Jean-Pierre Simorre , Catherine Bougault , Paul Schanda
{"title":"球菌细胞壁的 MAS NMR 实验:1H 和 CPMAS CryoProbe 增强 13C 检测实验的互补性","authors":"Alicia Vallet , Isabel Ayala , Barbara Perrone , Alia Hassan , Jean-Pierre Simorre , Catherine Bougault , Paul Schanda","doi":"10.1016/j.jmr.2024.107708","DOIUrl":null,"url":null,"abstract":"<div><p>Bacterial cell walls are gigadalton-large cross-linked polymers with a wide range of motional amplitudes, including rather rigid as well as highly flexible parts. Magic-angle spinning NMR is a powerful method to obtain atomic-level information about intact cell walls. Here we investigate sensitivity and information content of different homonuclear <sup>13</sup>C<img><sup>13</sup>C and heteronuclear <sup>1</sup>H<img><sup>15</sup>N, <sup>1</sup>H<img><sup>13</sup>C and <sup>15</sup>N<img><sup>13</sup>C correlation experiments. We demonstrate that a CPMAS CryoProbe yields ca. 8-fold increased signal-to-noise over a room-temperature probe, or a ca. 3–4-fold larger per-mass sensitivity. The increased sensitivity allowed to obtain high-resolution spectra even on intact bacteria. Moreover, we compare resolution and sensitivity of <sup>1</sup>H MAS experiments obtained at 100 kHz vs. 55 kHz. Our study provides useful hints for choosing experiments to extract atomic-level details on cell-wall samples.</p></div>","PeriodicalId":16267,"journal":{"name":"Journal of magnetic resonance","volume":null,"pages":null},"PeriodicalIF":2.0000,"publicationDate":"2024-06-06","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.sciencedirect.com/science/article/pii/S1090780724000922/pdfft?md5=80a76c4050d9dc251a1f625e0f15c7c5&pid=1-s2.0-S1090780724000922-main.pdf","citationCount":"0","resultStr":"{\"title\":\"MAS NMR experiments of corynebacterial cell walls: Complementary 1H- and CPMAS CryoProbe-enhanced 13C-detected experiments\",\"authors\":\"Alicia Vallet , Isabel Ayala , Barbara Perrone , Alia Hassan , Jean-Pierre Simorre , Catherine Bougault , Paul Schanda\",\"doi\":\"10.1016/j.jmr.2024.107708\",\"DOIUrl\":null,\"url\":null,\"abstract\":\"<div><p>Bacterial cell walls are gigadalton-large cross-linked polymers with a wide range of motional amplitudes, including rather rigid as well as highly flexible parts. Magic-angle spinning NMR is a powerful method to obtain atomic-level information about intact cell walls. Here we investigate sensitivity and information content of different homonuclear <sup>13</sup>C<img><sup>13</sup>C and heteronuclear <sup>1</sup>H<img><sup>15</sup>N, <sup>1</sup>H<img><sup>13</sup>C and <sup>15</sup>N<img><sup>13</sup>C correlation experiments. We demonstrate that a CPMAS CryoProbe yields ca. 8-fold increased signal-to-noise over a room-temperature probe, or a ca. 3–4-fold larger per-mass sensitivity. The increased sensitivity allowed to obtain high-resolution spectra even on intact bacteria. Moreover, we compare resolution and sensitivity of <sup>1</sup>H MAS experiments obtained at 100 kHz vs. 55 kHz. Our study provides useful hints for choosing experiments to extract atomic-level details on cell-wall samples.</p></div>\",\"PeriodicalId\":16267,\"journal\":{\"name\":\"Journal of magnetic resonance\",\"volume\":null,\"pages\":null},\"PeriodicalIF\":2.0000,\"publicationDate\":\"2024-06-06\",\"publicationTypes\":\"Journal Article\",\"fieldsOfStudy\":null,\"isOpenAccess\":false,\"openAccessPdf\":\"https://www.sciencedirect.com/science/article/pii/S1090780724000922/pdfft?md5=80a76c4050d9dc251a1f625e0f15c7c5&pid=1-s2.0-S1090780724000922-main.pdf\",\"citationCount\":\"0\",\"resultStr\":null,\"platform\":\"Semanticscholar\",\"paperid\":null,\"PeriodicalName\":\"Journal of magnetic resonance\",\"FirstCategoryId\":\"92\",\"ListUrlMain\":\"https://www.sciencedirect.com/science/article/pii/S1090780724000922\",\"RegionNum\":3,\"RegionCategory\":\"化学\",\"ArticlePicture\":[],\"TitleCN\":null,\"AbstractTextCN\":null,\"PMCID\":null,\"EPubDate\":\"\",\"PubModel\":\"\",\"JCR\":\"Q3\",\"JCRName\":\"BIOCHEMICAL RESEARCH METHODS\",\"Score\":null,\"Total\":0}","platform":"Semanticscholar","paperid":null,"PeriodicalName":"Journal of magnetic resonance","FirstCategoryId":"92","ListUrlMain":"https://www.sciencedirect.com/science/article/pii/S1090780724000922","RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":null,"EPubDate":"","PubModel":"","JCR":"Q3","JCRName":"BIOCHEMICAL RESEARCH METHODS","Score":null,"Total":0}
MAS NMR experiments of corynebacterial cell walls: Complementary 1H- and CPMAS CryoProbe-enhanced 13C-detected experiments
Bacterial cell walls are gigadalton-large cross-linked polymers with a wide range of motional amplitudes, including rather rigid as well as highly flexible parts. Magic-angle spinning NMR is a powerful method to obtain atomic-level information about intact cell walls. Here we investigate sensitivity and information content of different homonuclear 13C13C and heteronuclear 1H15N, 1H13C and 15N13C correlation experiments. We demonstrate that a CPMAS CryoProbe yields ca. 8-fold increased signal-to-noise over a room-temperature probe, or a ca. 3–4-fold larger per-mass sensitivity. The increased sensitivity allowed to obtain high-resolution spectra even on intact bacteria. Moreover, we compare resolution and sensitivity of 1H MAS experiments obtained at 100 kHz vs. 55 kHz. Our study provides useful hints for choosing experiments to extract atomic-level details on cell-wall samples.
期刊介绍:
The Journal of Magnetic Resonance presents original technical and scientific papers in all aspects of magnetic resonance, including nuclear magnetic resonance spectroscopy (NMR) of solids and liquids, electron spin/paramagnetic resonance (EPR), in vivo magnetic resonance imaging (MRI) and spectroscopy (MRS), nuclear quadrupole resonance (NQR) and magnetic resonance phenomena at nearly zero fields or in combination with optics. The Journal''s main aims include deepening the physical principles underlying all these spectroscopies, publishing significant theoretical and experimental results leading to spectral and spatial progress in these areas, and opening new MR-based applications in chemistry, biology and medicine. The Journal also seeks descriptions of novel apparatuses, new experimental protocols, and new procedures of data analysis and interpretation - including computational and quantum-mechanical methods - capable of advancing MR spectroscopy and imaging.